Method of manufacturing hydrogen sulphide gas



Patented Dec. 15,. 1 925.

" P N Q' acE;-*=

MIDEEINDS HEDLER, E LANsDOWNE, 1 ENNsYLvANIA, AND EDWARD w. EUGE- LEY, 0F HODEWELL, vInGrNrA, AssIGNons 0E THEIR ENTIRE RIGHT TO ITUBIZ ABTIFICIAL;SILK comr NY 0E AMEnIcA, A coRroaArIoN' OF DELAWAR A ,KEIHOD OF MANUFACTURING HYDROGEN SULPI-IIDE GAS.

To all whom it may concern.

Be it known that we, E'MILE-BINosoHED- v LER, a citizen of the Republic of Switzerland, and resident of Lansdowne, in the 5 county of Delaware, in the State of Pennsylvania, and EDWARD W. R'UGELEY, a citizen of the United States of America, and

resident of Hopewell, county of Prince tion of generating hydrogen sulphide gas by heating. sulphur with tar oil .or petroleum products like Mexican crude oil, heavy petroleum oil, paraflin oil and asphalt.

- If'sulphu'r is, for instance, heated with l heavyiuel. oil, which is especially well adapted for the urpose; the. generation of hydrogen sulphi e gas starts already at a relatively low temperature around'125. 0;, and proceeds rather rapidly between 200 and 300 C. When the heated mixture attains atemperature of about 200 0., cracking of the oilsoccurs and while the resultant vaporized products such as gasoline and kerosene can be condensed and recovered in 3 any convenient way, we prefer to carry out the process under reflux so that these hydrocarbons are condensed and returned to the heated vessel containing the mixture under treatment so as to make them available for 4 reaction with sulphur. This reflux reaction has also the advantage of carrying back any vaporized sulphur which otherwise would sublime over. The eflfect of carrying out our process under reflux enables us to. use proportions of one part of sulphur to about .875 of oils without impair ng the yield of hydrogen sulphide gas.

In order to complete the reaction and to obtain the highest possible yield, we found it necessary to raise the temperature of the mixture of sulihur and hydrocarbon oils to nearly 400 We have now found that when the temperature reaches about 350 C.

ollowing is. a

- removed Application filed April 15, 1924. Serial No."706,716.

mercaptane compounds of an. obnoxious odor are formed contaminating the hydrogen sulphide gas. duced, for instance, into-sodium sulphide solution, caustic soda 1 e or milk of lime for-the purpose of ma 'ng sulphhydrates, the obnoxious odor pertains to the solution andmakes it not only very unpleasant to If the latter is introhandle, but almost unfit for use in denitrating nitrocellulose silk.

We have now dlscovered that hydrogen sulphide gas can be purified from these mercaptane products by passing it through certain materials of high absorptive capacity like silica gel, activated carbon,'coke or charcoal. These materials absorb the mercaptane compounds leaving only pure hydrogen sulphide gas Whichwhen introduced into appropriate absorption liquids, yields 5 sulphhydrate solutions of great purity and free from any obnoxious odor; Charcoal is very well adapted for the purpose and being very cheap.

The following are two examples of the practical employment of our process:

' First. 1,000 pounds sulphur and 1,500

.pounds heavy Mexican fuel oil are mixed.

in an; iron kettle provided with a stirring arrangement and gradually heated until a temperature of 400 C..is reached and the generation of hydrogen sulphide gas ceases.

has the advantage over other materials of I During the reaction about 500 pounds of v gasolineand kerosene'products distill over andare condensed by cooling. The hydrogen sulphide gas passes first through a container with cracked oil to retain sulphur and then through one or several cooled containers filled with charcoal; and is after wards either liquefied or .worked up into known methods. After the charcoal has 'sulphhydrate solutions according to well 9 5 lost its absorptive capacity for the mer- I captane impurities, it can be reactivated by j superheated steam. Goke'formed as a by-';.-- product during the reactionbetween hydro-' carbon oils and sulphur is obtained in high 1 purity in' ulverized form and can easilyjbe om the'kettle and used for the, making of bricks, by mixing it with crude 7 oil or asphalt and pressing it or for making I of producer. purposes oro OI'WISO-I'.

or as such'for reduction Second. 875 pounds of crude'oil previously heated to 200 C. are loaded in an iron kettle provided withstirring arrangement and a reflux condenser or air cooler with bafiie plates. 1,000 pounds of molten sulphur are then gradually introduced and the what we claim as new and desire tosecure by Letters Pat ent, is:

l. The method of manufacturing hydrogen sulphide gas which consists in heating a mixture of hydrocarbon oils and'sulphur and purifying the hydrogen sulphide gas evolved by this treatment by passing it through a material of high absorptive capacit 2. The method of manufacturing hydrogen sulphide gas which consists in heating a mixture of hyrdocarbon oils and sulphur under reflux to prevent cracked oil products from distilling over and purifying the hydrogen sulphide gas evolved by this treatment by passing it through a material of high absorptive capacity.

3. The method of manufacturing hydrogen sulphide gas which consists in heating a mixture of hydrocarbon oils and sulphur at a temperature between 200 and 400 C. and purifying the hydrogen sulphide gas evolved by this treatment by passing it through a material of high absorptive capacity. Y v I 4.'The method of manufacturing hydrogen sulphide gas Which consists in'heating a mixture of hydrocarbon oils and sulphur and purifying the hydrogen sulphide gas evolved by this treatment by passing it' through a carbonaceous material of high absorptive capacity.

5. The method of manufacturing hydrogen sulphide a mixture of petroleum oils and sulphur under reflux to prevent cracked oil products from distilling over and purifying the hydrogen sulphide gas evolved by this treatment by p'assing it through a material of high absorptive capacity.

6. The method of manufacturing hydrogen sulphide gas which consists in heating a heavy fuel oil to a temperature of about 200 C., gradually introducing sulphur into the heated oil in about the proportion of one part of sulphur to from .8 to 1.2 parts of oil, raising the temperature of the mixture to from about 350 to 400 C.-under reflux and purifying the hydrogen sulphide gas evolved by passing it through carbo naceous material of; high absorptive capacity.

7. In the method of claim 1, the use of charcoal under cooling as the absorbent material.

8. In the method of claim 6, the use of charrioal under cooling as the absorbent materia EMILE BINDSCHEDLER. EDWARD w. RUGELEY.

gaswhich consists in heating 

